EP0266769A2 - Cellule à écoulement pour photomètre - Google Patents

Cellule à écoulement pour photomètre Download PDF

Info

Publication number
EP0266769A2
EP0266769A2 EP87116310A EP87116310A EP0266769A2 EP 0266769 A2 EP0266769 A2 EP 0266769A2 EP 87116310 A EP87116310 A EP 87116310A EP 87116310 A EP87116310 A EP 87116310A EP 0266769 A2 EP0266769 A2 EP 0266769A2
Authority
EP
European Patent Office
Prior art keywords
liquid sample
flow cell
groove
cell body
light
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP87116310A
Other languages
German (de)
English (en)
Other versions
EP0266769B1 (fr
EP0266769A3 (en
Inventor
Masao Kamahori
Yoshio Watanabe
Junkichi Miura
Mamoru Taki
Hiroyuki Miyagi
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hitachi Ltd
Original Assignee
Hitachi Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hitachi Ltd filed Critical Hitachi Ltd
Publication of EP0266769A2 publication Critical patent/EP0266769A2/fr
Publication of EP0266769A3 publication Critical patent/EP0266769A3/en
Application granted granted Critical
Publication of EP0266769B1 publication Critical patent/EP0266769B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0346—Capillary cells; Microcells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • G01N2021/054—Bubble trap; Debubbling
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • G01N2030/746—Optical detectors detecting along the line of flow, e.g. axial
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors

Definitions

  • This invention relates to a flow cell for a photometer, and particularly to a flow cell for a photometer suitable for a liquid chromatographic detector.
  • a conventional flow cell for an optical detector comprises a plate-shaped, flow cell body provided with a light path perforation at the center and with a liquid sample inlet passage and a liquid sample outlet passage at both ends of the perforation, and a pair of window members joined at both sides of the plate-shaped, flow cell body, where the flow cell is made smaller in size and the diffusion of liquid sample bands is reduced, as disclosed in Japanese Patent Application Kokai (Laid-open) No. 60-125540.
  • This conventional flow cell has a very small flow cell (cuvette) volume, e.g.
  • this conventional flow cell has a very low measurement effect.
  • the conven­tional flow cell also proposes to use the reflected light, but use of the reflected light leads to a noise increase, but there is no disclosure of noise reduction in this prior art literature.
  • An object of the present invention is to provide a flow cell of light transmission type for a photometer, where the unwanted disturbance in the liquid sample flow is thoroughly suppressed.
  • Another object of the present invention is to provide a flow cell of light transmission type for a photometer, where the dead volume or the unwanted disturb­ance in the liquid sample flow is reduced by forming a light path and liquid sample flow passages in appropriate shapes in the flow cell, finely polishing the inner surfaces of the light path and liquid sample flow passages, and particularly providing a light reflecting layer on the light path to the full length.
  • a flow cell for a photometer which comprises a cell body integrated from a pair of cell body members by joining, at least one of which is provided with a linear groove on the joining surface of the cell body member from one end to another to the full length, as exposed to the bonding surface, the groove playing both roles of a liquid sample passage and a detecting light path by the integration of the cell body members, and is further provided with a liquid sample inlet passage at a position near one end of the groove and a liquid sample outlet passage at a position near the other end of the groove, both passages being communicated with the groove, and a pair of light transmission window members joined with the flow cell body at both ends on the groove-open sides thereof.
  • the linear grooves can be provided on the joining surfaces of both cell body members from one end to the other to the full length, symmetrically to each other and exposed to the joining surfaces.
  • a light reflecting layer is preferably provided on the surfaces of linear grooves to the full length.
  • the liquid sample inlet passage and the liquid sample outlet passage are preferably provided on at least one of the joining surfaces of cell body members, as exposed to the joining surface and communicated with the first linear groove.
  • the light path can be formed by forming a straight groove on at least one of the joining surfaces, as exposed to the joining surface, and joining the cell body members, the groove can be readily polished or a light reflecting layer can be readily formed on the groove before joining the cell body members.
  • random light reflection on the flow cell inside or light absorption due to poor reflection can be reduced and also the disturbance in the liquid sample flow through the light path can be suppressed.
  • fabrication of a flow cell itself can be readily made.
  • the liquid sample inlet passage and the liquid sample outlet passage can be likewise formed on at least one of the joining surfaces of cell body members, as exposed to the joining surface, and thus their shapes suitable for reducing the disturbance in the liquid sample flow through the light path can be readily and appropriately formed or their surfaces can be readily and finely polished.
  • Fig. 1 shows an assembled flow cell for a photo­meter according to the present invention.
  • the flow cell comprises a pair of cell body members 1 and 1 ⁇ and light transmission window members 2 and 2 ⁇ and has liquid sample inlet and outlet passages 4 and 4 ⁇ and a light path 3 through which a liquid sample and a detecting light can pass.
  • Fig. 2 is views showing assembling of the flow cell.
  • light path grooves 5 and 5 ⁇ are formed on the joining surfaces of cell body members 1 and 1 ⁇ , respectively, and liquid sample inlet passage and outlet passage 4 and 4 ⁇ are formed in the cell body members 1 and 1 ⁇ , respectively.
  • the grooves 5 and 5 ⁇ are formed by tightly joining and fixing a pair of the cell body members 1 and 1 ⁇ , and making a perforation along the joining surfaces at the center to the full length by a drill. After the formation of the perforation, the cell body members 1 and 1 ⁇ are separated from each other, and the resulting linear grooves 5 and 5 ⁇ on the respective joining faces are polished by lapping or chemical polishing.
  • the cell body members 1 and 1 ⁇ are joined together by firm bonding, whereby a circular light path 3 is formed, as shown in Fig. 2B.
  • the grooves 5 and 5 ⁇ are formed by tightly joining and fixing the two cell body members 1 and 1 ⁇ by drilling, the joining of the polished grooves 5 and 5 ⁇ can be carried out with high precision only by aligning the contours of the cell body members 1 and 1 ⁇ .
  • liquid sample flow passages 4 and 4 ⁇ are made by a drill.
  • the cell body members 1 and 1 ⁇ and the light transmission members 2 and 2 ⁇ are composed of quartz glass.
  • the cell body members 1 and 1 ⁇ may be composed of other glass, e.g. soda glass, silicon, or silicon oxide.
  • the joining surfaces of the cell body members 1 and 1 ⁇ can be bonded together by melt bonding such as anodic bonding, or occasionally by smoothing the bonding surfaces and pressure bonding the joining surfaces, such as optical contact, to form a flow cell. No liquid leakage occurs at the joints of the bonding surfaces.
  • Fig. 3 shows an assembly of a flow cell for a photometer according to the present invention, where the flow cell comprises a pair of cell body members 11 and 11 ⁇ and light transmission window members 12 and 12 ⁇ and has liquid sample inlet passage 14 and outlet passage 14 ⁇ and a light path through which a liquid sample and a detecting light pass.
  • the structure of the flow cell is different from that of Figs. 2A and 2B only in that the liquid sample inlet passage 14 and outlet passage 14 ⁇ are formed on the respective joining surfaces of cell body members, as exposed to the joining surfaces and communicated with the straight light path grooves, as shown in Figs. 4A and 4B.
  • Figs. 5A and 5B show a schematic view of assem­bling a flow cell having a light reflecting layer on the grooves and a cross-sectional view of the flow cell according to the present invention, respectively.
  • liquid sample inlet passage 24 and outlet passage 24 ⁇ are provided on cell body members 21 and 21 ⁇ , respectively, as communicated with light path grooves 25 and 25 ⁇ , respectively, whereas the light path grooves 25 and 25 ⁇ are formed on the joining surfaces of cell body members 21 and 21 ⁇ , respectively, as exposed to the joining surfaces.
  • a light reflecting layer 26 is formed on the surfaces of the light path grooves 25 and 25 ⁇ .
  • the light reflecting layer 26 can be formed on the grooves 25 and 25 ⁇ by vacuum vapor deposition, by electron beam vapor deposition by allowing an electron beam to hit a sample in vacuum, thereby elevating the temperature of the sample and facilitating vapor deposition, or by sputtering by generating a plasma from an argon gas, sputtering a sample with the generated Ar+, thereby physically scraping the sample.
  • the light reflecting layer 26 is composed of a glass having a lower refractive index than that of the solvent in the liquid sample, or a metal of high reflectivity such as aluminum, rhodium, etc. In the case of aluminum light reflecting layer, the layer is coated with silicon oxide to give a corrosion resistance thereto.
  • the cell body members 21 and 21 ⁇ are joined together and light trans­mission window members 22 and 22 ⁇ are bonded to both ends of cell body to form a flow cell, as shown in Fig. 5B.
  • the light reflecting layer can be likewise formed on the surfaces of grooves of embodiments of Figs. 1 and 2 and Figs. 3 and 4.
  • the following Table shows noise test results of flow cells according to the present invention and a conventional flow cell whose light path was fabricated by drilling, as in, for example, said Japanese Patent Application Kokai (Laid-open) No. 60-125540. Tests were carried out under the following conditions: Cell volume : 0.6 ⁇ l (inner diameter: 0.5 mm; light path length: 3 mm) Detecting wavelength : 250 nm
  • Air or methanol was passed through the cell during the test.
  • flow rate of methanol was 0.1 ml/min.
  • noise could be reduced by polishing the inside surface, thereby reducing the irregularities of the flow cell inside surface. Furthermore, the noise was further reduced in a flow cell provided with a light reflecting layer on the light path inside surface by vacuum vapor depositing aluminum on the inside surface, and with a further SiO2 layer thereon through electron beam vapor deposition, i.e. by allowing an electron beam to hit a SiO2 sample, thereby elevating the temperature, thereby vacuum vapor deposition of SiO2 onto the aluminum layer, to a total layer thickness of 2,000 ⁇ , and thus the effect by the light reflecting layer is evident.
  • Fig. 6 is cross-sectional views of flow cells according to the present invention, where Fig. 6A shows that liquid sample inlet passage 24 and outlet passage 24 ⁇ , and a light path 23 are rounded at their joints, and Fig. 6B shows that liquid sample inlet passage 28 and outlet passage 28 ⁇ are in a S shape. According to the rounded joints and rounded shapes of the liquid sample inlet and outlet passages, diffusion of liquid sample bands can have been made lower in the flow cell for the first time.
  • Cell body members 21 and light transmission window members 22 and 22 ⁇ are the same as used in the embodiment of Fig. 5.
  • FIG. 7 Further embodiment of the present flow cell is shown in Fig. 7 by way of its assembling, where a light path groove 36 and S-shaped liquid sample inlet passage 35 and outlet passage 35 ⁇ are formed only on the joining surface of a cell body member 31 composed of quartz glass. Then, the cell body member 31 is joined with another cell body member 32 without any groove thereon, and a pair of light transmission window members (not shown in the draw­ing) are bonded to both ends of the flow cell body at the groove-open sides to form a flow cell having a light path 36 and liquid sample inlet passage 35 and outlet passage 35 ⁇ .
  • Fig. 8 shows cross-sectional views of light path grooves and liquid sample passage of various shapes.
  • Fig. 8A shows a half-circle groove 42
  • Fig. 8B a square groove 43
  • Fig. 8C a triangular groove 44 , each on a cell body member 41 .
  • a groove of any other shape can be also used.
  • a liquid chromatograph comprises an eluting solution tank 51 for storing an eluting solution as a carrier, a pump for feeding the eluting solution from the tank 51 , a sample injector 53 for introducing a mixed sample into the eluting solution, a separation column 54 for separating sample components as introduced, a spectrophotometer for detecting the sample components separated in the column 54 and a recorder 56 for recording output from the spectrophotometer 55 .
  • the spectrophotometer 55 is shown in Fig. 10, and comprises a light source 57 , a light-collecting mirror 58 for collecting the light emitted from the light source 57 , a diffraction lattice 59 for spectrolyzing the light collected on the mirror 58 , a flow cell 66 through which the eluate from the separation column 54 as a liquid sample passes and also the spectrolyzed beam from the diffraction lattice 51 passes straight, a photodiode 61 for detecting the light that has passed through the flow cell 60 and a detection circuit 62 for converting the output from the photodiode 61 to a voltage.
  • the inside surfaces of the light path and liquid sample passages can be readily polished and thus the dead volume or disturbance in the liquid sample flow through the flow cell can be suppressed.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Optical Measuring Cells (AREA)
EP87116310A 1986-11-07 1987-11-05 Cellule à écoulement pour photomètre Expired - Lifetime EP0266769B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP26378386 1986-11-07
JP263783/86 1986-11-07

Publications (3)

Publication Number Publication Date
EP0266769A2 true EP0266769A2 (fr) 1988-05-11
EP0266769A3 EP0266769A3 (en) 1990-01-24
EP0266769B1 EP0266769B1 (fr) 1993-05-19

Family

ID=17394206

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87116310A Expired - Lifetime EP0266769B1 (fr) 1986-11-07 1987-11-05 Cellule à écoulement pour photomètre

Country Status (4)

Country Link
US (1) US4823168A (fr)
EP (1) EP0266769B1 (fr)
JP (1) JPS63241337A (fr)
DE (1) DE3785909T2 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0396163A3 (fr) * 1989-04-14 1991-02-27 Kontron Instruments Holding N.V. Cuve de chasse capillaire
DE4004990A1 (de) * 1990-02-19 1991-08-22 Rosemount Gmbh & Co Analysenkuevette
EP0762119A1 (fr) * 1995-09-06 1997-03-12 Hewlett-Packard GmbH Dispositif photométriques pour des échantillons à volume faible
GB2312745A (en) * 1996-05-03 1997-11-05 Intevep Sa Determining a parameter of a substance, especially a hydrocarbon
WO2004090513A1 (fr) * 2003-04-10 2004-10-21 Endress+Hauser Conducta Gesellschaft Für Mess- Und Regeltechnik Mbh + Co. Kg Dispositif de mesure photometrique de la concentration d'une substance chimique dans une solution de mesure
EP1626266A4 (fr) * 2003-05-13 2012-02-01 Gl Sciences Inc Cuve a circulation comprenant un tube capillaire
EP2927670A4 (fr) * 2012-11-30 2015-10-28 Panasonic Ip Man Co Ltd Appareil de capteur optique et procédé de fabrication d'élément optique à utiliser dans un appareil de capteur optique

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US5747349A (en) * 1996-03-20 1998-05-05 University Of Washington Fluorescent reporter beads for fluid analysis
JP2005504317A (ja) 2001-09-28 2005-02-10 イビディ ゲムベーハー フロー・チャンバー
US7029631B2 (en) * 2002-04-19 2006-04-18 Agilent Technologies, Inc. Apparatus for improved light collection
US6741348B2 (en) 2002-04-29 2004-05-25 The Curators Of The University Of Missouri Ultrasensitive spectrophotometer
US7294839B2 (en) * 2002-10-08 2007-11-13 Ric Investements, Inc. Low volume sample cell and gas monitoring system using same
US6867857B2 (en) 2002-10-29 2005-03-15 Nanostream, Inc. Flow cell for optical analysis of a fluid
WO2004040295A1 (fr) * 2002-10-31 2004-05-13 Nanostream, Inc. Systemes de chromatographie de detection en parallele
US7050660B2 (en) * 2003-04-07 2006-05-23 Eksigent Technologies Llc Microfluidic detection device having reduced dispersion and method for making same
US7268881B2 (en) * 2004-02-17 2007-09-11 The Curators Of The University Of Missouri Light scattering detector
US20050257885A1 (en) * 2004-05-24 2005-11-24 Nanostream, Inc. Capillary multi-channel optical flow cell
US7189960B2 (en) * 2004-08-27 2007-03-13 The Toro Company Optical moisture sensor
US7903252B2 (en) * 2005-01-13 2011-03-08 The Curators Of The University Of Missouri Noise cancellation in fourier transform spectrophotometry
US7262844B2 (en) * 2005-01-13 2007-08-28 The Curators Of The University Of Missouri Ultrasensitive spectrophotometer
CN101755204A (zh) 2006-03-09 2010-06-23 全技术联合公司 蒸发光散射检测器
CN100419406C (zh) * 2006-03-31 2008-09-17 洪陵成 流动光度分析流通池
US7545490B1 (en) * 2006-09-26 2009-06-09 Itt Manufacturing Enterprises, Inc. Microscope flow cell apparatus for raman analysis of a liquid
EP2124036A1 (fr) 2008-05-20 2009-11-25 Agilent Technologies, Inc. Pré-positionnement et mécanisme de guidage pour insérer une cellule à flot continu dans un détecteur
WO2009152321A1 (fr) * 2008-06-11 2009-12-17 The Curators Of The University Of Missouri Détecteur de chromatographie en phase liquide et régulateur de débit pour ledit détecteur
JP2010060484A (ja) * 2008-09-05 2010-03-18 Yazaki Corp 気体セル、気体サンプル室、及び、濃度測定装置
US8233146B2 (en) * 2009-01-13 2012-07-31 Becton, Dickinson And Company Cuvette for flow-type particle analyzer
US8502969B2 (en) * 2009-12-16 2013-08-06 Boule Medical Ab Miniature flow-through cuvette and spectrophotometer containing the same
US9007050B2 (en) 2010-09-17 2015-04-14 The Toro Company Soil moisture sensor with improved enclosure
US8981946B2 (en) 2011-10-24 2015-03-17 The Toro Company Soil moisture sensor
WO2016154578A1 (fr) * 2015-03-25 2016-09-29 Eta Diagnostics, Inc. Cellule optique construite par liaison par voie anodique d'une couche métallique mince entre deux fenêtres en verre optiquement transparent
US10871440B2 (en) 2017-12-23 2020-12-22 Lumacyte, LLC Microfluidic chip device for optical force measurements and cell imaging using microfluidic chip configuration and dynamics
CN119281410A (zh) * 2017-12-23 2025-01-10 路玛赛特有限责任公司 利用微流控芯片构型和动力学进行光力测量和细胞成像的微流控芯片设备
US11041797B2 (en) 2017-12-23 2021-06-22 Lumacyte, LLC Microfluidic chip device for optical force measurements and cell imaging using microfluidic chip configuration and dynamics
EP3647769A1 (fr) 2018-10-29 2020-05-06 ETH Zurich Cellule d'écoulement
WO2021159458A1 (fr) * 2020-02-14 2021-08-19 科宝智慧医疗科技（上海）有限公司 Contenant pour l'analyse de liquide
CN115656047B (zh) * 2022-09-27 2025-09-12 大连依利特分析仪器有限公司 横截面异形渐变双轴向锥型腔流动池
WO2025259818A1 (fr) * 2024-06-12 2025-12-18 Bennubio, Inc. Structures usinées dans des cellules à flux acousto-optique à couches métalliques minces liées de manière anodique
DE102024124093A1 (de) * 2024-08-22 2026-02-26 Endress+Hauser Conducta Gmbh+Co. Kg Messzelle

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5141548A (en) * 1986-04-14 1992-08-25 Kontron Instruments Holding Nv Method of manufacturing a capillary flow cell
EP0396163A3 (fr) * 1989-04-14 1991-02-27 Kontron Instruments Holding N.V. Cuve de chasse capillaire
US5057216A (en) * 1989-04-14 1991-10-15 Kontron Instruments Holding Nv Capillary flow cell
DE4004990C2 (de) * 1990-02-19 1998-04-09 Fisher Rosemount Gmbh & Co Ges Analysenküvette
DE4004990A1 (de) * 1990-02-19 1991-08-22 Rosemount Gmbh & Co Analysenkuevette
EP0762119A1 (fr) * 1995-09-06 1997-03-12 Hewlett-Packard GmbH Dispositif photométriques pour des échantillons à volume faible
US5917606A (en) * 1995-09-06 1999-06-29 Hewlett-Packard Company Photometric flow apparatus for small sample volumes and method of making same
GB2312745A (en) * 1996-05-03 1997-11-05 Intevep Sa Determining a parameter of a substance, especially a hydrocarbon
GB2312745B (en) * 1996-05-03 2000-10-11 Intevep Sa Apparatus for determining a parameter of a substance, especially a hydrocarbon
WO2004090513A1 (fr) * 2003-04-10 2004-10-21 Endress+Hauser Conducta Gesellschaft Für Mess- Und Regeltechnik Mbh + Co. Kg Dispositif de mesure photometrique de la concentration d'une substance chimique dans une solution de mesure
EP1626266A4 (fr) * 2003-05-13 2012-02-01 Gl Sciences Inc Cuve a circulation comprenant un tube capillaire
EP2927670A4 (fr) * 2012-11-30 2015-10-28 Panasonic Ip Man Co Ltd Appareil de capteur optique et procédé de fabrication d'élément optique à utiliser dans un appareil de capteur optique
US9651475B2 (en) 2012-11-30 2017-05-16 Panasonic Intellectual Property Management Co., Ltd. Optical sensor apparatus and method of producing optical element used in optical sensor apparatus

Also Published As

Publication number Publication date
JPS63241337A (ja) 1988-10-06
DE3785909T2 (de) 1993-11-18
DE3785909D1 (de) 1993-06-24
US4823168A (en) 1989-04-18
JPH0583141B2 (fr) 1993-11-24
EP0266769B1 (fr) 1993-05-19
EP0266769A3 (en) 1990-01-24

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